JP7432804B2 - Fiber treatment agent for nonwoven fabric production and its use - Google Patents
Fiber treatment agent for nonwoven fabric production and its use Download PDFInfo
- Publication number
- JP7432804B2 JP7432804B2 JP2023567222A JP2023567222A JP7432804B2 JP 7432804 B2 JP7432804 B2 JP 7432804B2 JP 2023567222 A JP2023567222 A JP 2023567222A JP 2023567222 A JP2023567222 A JP 2023567222A JP 7432804 B2 JP7432804 B2 JP 7432804B2
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- Japan
- Prior art keywords
- compound
- treatment agent
- acid
- nonwoven fabric
- fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000835 fiber Substances 0.000 title claims description 117
- 239000004745 nonwoven fabric Substances 0.000 title claims description 93
- 239000003795 chemical substances by application Substances 0.000 title claims description 75
- 238000004519 manufacturing process Methods 0.000 title claims description 40
- 150000001875 compounds Chemical class 0.000 claims description 136
- 229910052816 inorganic phosphate Inorganic materials 0.000 claims description 33
- 125000004432 carbon atom Chemical group C* 0.000 claims description 30
- 239000002253 acid Substances 0.000 claims description 26
- 125000000217 alkyl group Chemical group 0.000 claims description 18
- 229910052783 alkali metal Inorganic materials 0.000 claims description 13
- 150000001340 alkali metals Chemical class 0.000 claims description 13
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000003755 preservative agent Substances 0.000 claims description 3
- 230000002335 preservative effect Effects 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 description 54
- -1 phosphoric acid compound Chemical class 0.000 description 44
- 238000005481 NMR spectroscopy Methods 0.000 description 27
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- 235000014113 dietary fatty acids Nutrition 0.000 description 20
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- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 4
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- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- QAEVVAMQWJMMGX-UHFFFAOYSA-M sodium;didodecyl phosphate Chemical compound [Na+].CCCCCCCCCCCCOP([O-])(=O)OCCCCCCCCCCCC QAEVVAMQWJMMGX-UHFFFAOYSA-M 0.000 description 1
- JDSVWTAJRNTSSL-UHFFFAOYSA-M sodium;dodecyl hydrogen phosphate Chemical compound [Na+].CCCCCCCCCCCCOP(O)([O-])=O JDSVWTAJRNTSSL-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000001593 sorbitan monooleate Substances 0.000 description 1
- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
- 229940035049 sorbitan monooleate Drugs 0.000 description 1
- 235000019337 sorbitan trioleate Nutrition 0.000 description 1
- 229960000391 sorbitan trioleate Drugs 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- ORLIFRJRAMADMX-MSUUIHNZSA-N tridecyl (z)-octadec-9-enoate Chemical compound CCCCCCCCCCCCCOC(=O)CCCCCCC\C=C/CCCCCCCC ORLIFRJRAMADMX-MSUUIHNZSA-N 0.000 description 1
- INJZMNQWJIWOEA-UHFFFAOYSA-N tridecyl dodecanoate Chemical compound CCCCCCCCCCCCCOC(=O)CCCCCCCCCCC INJZMNQWJIWOEA-UHFFFAOYSA-N 0.000 description 1
- QEIJVPZRDAHCHE-UHFFFAOYSA-N tridecyl hexadecanoate Chemical compound CCCCCCCCCCCCCCCC(=O)OCCCCCCCCCCCCC QEIJVPZRDAHCHE-UHFFFAOYSA-N 0.000 description 1
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 description 1
- 229910000404 tripotassium phosphate Inorganic materials 0.000 description 1
- 235000019798 tripotassium phosphate Nutrition 0.000 description 1
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 1
- 235000019801 trisodium phosphate Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000011041 water permeability test Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
- D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Description
本発明は、不織布製造用繊維処理剤及びその利用に関する。 The present invention relates to a fiber treatment agent for producing nonwoven fabrics and its use.
従来から、短繊維を不織布に加工する場合、カード工程が行われる。しかし、短繊維がカードを通過する際に静電気発生量が多い若しくはカード通過性が良好でないと、ウェブが均一でなくなり、不織布の厚さに斑が生じる原因になる。したがって、静電気発生の抑制及び良好なカード通過性を付与することができる繊維処理剤が使用されている。
また、一般に、紙おむつや合成ナプキンを代表とする生理用品等の吸収性物品に用いられる少なくとも1種の熱可塑性樹脂を含む繊維(ポリオレフィン系繊維、ポリエステル系繊維等)を主材とする各種不織布に親水性を付与したトップシートと、撥水性を付与したバックシートと、トップシートとバックシートの間に綿状パルプや高分子吸収体等からなる材料とを配置した3層から形成される構造になっていることが多い。尿や体液等の液体はトップシートを通過して吸収体に吸収されるが、トップシートには透水性のよいこと、すなわち液体がトップシート上から内部の吸収体に完全に吸収される迄の時間が極めて短い瞬時透水性が必要である。さらに、僅か1回から2回の液体の吸収によってトップシート上の処理剤が流出して透水性が急激に低下するのは、おむつの取り替え回数が増すことになって好ましくないので、トップシートには繰り返しの液体吸収に耐える耐久透水性が要求される。
不織布製造用繊維処理剤の耐久透水性を向上するために、高分子化合物を含む処理剤が提案されている(特許文献1)。
Conventionally, when processing short fibers into nonwoven fabrics, a carding process is performed. However, if a large amount of static electricity is generated when the short fibers pass through the card, or if the card passing property is not good, the web will not be uniform and the thickness of the nonwoven fabric will be uneven. Therefore, fiber treatment agents are used that can suppress the generation of static electricity and provide good card passage properties.
In addition, various types of nonwoven fabrics based on fibers containing at least one type of thermoplastic resin (polyolefin fibers, polyester fibers, etc.) are generally used in absorbent articles such as sanitary products such as disposable diapers and synthetic napkins. The structure is made up of three layers: a top sheet with hydrophilic properties, a back sheet with water repellency, and a material made of cotton pulp or polymeric absorbent between the top sheet and the back sheet. This is often the case. Liquids such as urine and body fluids pass through the top sheet and are absorbed by the absorbent body, but the top sheet has good water permeability. Instant water permeability is required for an extremely short period of time. Furthermore, it is undesirable for the treatment agent on the top sheet to flow out after just one or two liquid absorptions, resulting in a sudden drop in water permeability, which increases the number of diaper changes. requires durable water permeability that can withstand repeated liquid absorption.
In order to improve the durable water permeability of a fiber treatment agent for producing nonwoven fabrics, a treatment agent containing a polymer compound has been proposed (Patent Document 1).
高分子化合物を含む不織布製造用繊維処理剤が付与された不織布は、確かに耐久親水性は優れるものの、経時的に親水性が低下するという問題が見られるようになった。
本発明が解決しようとする課題は、高温経時後に親水性が低下しない不織布製造用繊維処理剤及び用いた短繊維を提供することである。
Nonwoven fabrics to which a fiber treatment agent for producing nonwoven fabrics containing a polymer compound has been applied certainly have excellent durable hydrophilicity, but a problem has arisen in that the hydrophilicity decreases over time.
The problem to be solved by the present invention is to provide a fiber treatment agent for nonwoven fabric production that does not lose its hydrophilicity after aging at high temperatures, and short fibers used therein.
本発明者等は、前記課題を解決するために鋭意検討した結果、特定の燐酸化合物を特定量含有し、その酸価が一定の値を示す不織布製造用繊維処理剤であれば、解決できることを突き止めた。
すなわち、本発明の不織布製造用繊維処理剤は、下記一般式(1)で示される化合物(A)、下記一般式(2)で示される化合物(B)、下記一般式(3)で示される化合物(C)及び無機燐酸塩(IN)から選ばれる少なくとも1種を含む不織布製造用繊維処理剤であって、前記化合物(A)、前記化合物(B)及び前記化合物(C)を必須に含み、処理剤の不揮発分に対して、前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)の合計重量割合が80~100重量%であり、前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)のそれぞれに帰属されるP核NMR積分値の合計(A+B+C+IN)に対して、前記化合物(A)に帰属されるP核NMR積分値(A)の比率〔A/(A+B+C+IN)〕が20~50%、前記化合物(B)に帰属されるP核NMR積分値(B)の比率〔B/(A+B+C+IN)〕が20~50%、前記化合物(C)に帰属されるP核NMR積分値(C)の比率〔C/(A+B+C+IN)〕が20~50%であり、前記処理剤の不揮発分の酸価(KOHmg/g)が100未満である。
As a result of intensive studies to solve the above problem, the present inventors have found that the problem can be solved by a fiber treatment agent for nonwoven fabric production that contains a specific amount of a specific phosphoric acid compound and has a certain acid value. I figured it out.
That is, the fiber treatment agent for nonwoven fabric production of the present invention comprises a compound (A) represented by the following general formula (1), a compound (B) represented by the following general formula (2), and a compound represented by the following general formula (3). A fiber treatment agent for nonwoven fabric production containing at least one selected from compound (C) and inorganic phosphate (IN), which essentially contains the compound (A), the compound (B), and the compound (C). , the total weight proportion of the compound (A), the compound (B), the compound (C) and the inorganic phosphate (IN) is 80 to 100% by weight based on the nonvolatile content of the treatment agent, and the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN), with respect to the total (A+B+C+IN) of the P-nuclear NMR integral values assigned to the compound (A). The ratio of the P-nuclear NMR integral value (A) assigned to the compound (B) [A/(A+B+C+IN)] is 20 to 50%, and the ratio of the P-nuclear NMR integral value (B) assigned to the compound (B) [B/(A+B+C+IN)] ] is 20 to 50%, the ratio [C/(A+B+C+IN)] of the P nuclear NMR integral value (C) attributed to the compound (C) is 20 to 50%, and the acid value of the nonvolatile content of the processing agent is 20 to 50%. (KOHmg/g) is less than 100.
(式(1)中、R1は直鎖の炭素数12のアルキル基、Q1は、直鎖の炭素数12のアルキル基、アルカリ金属又は水素原子を示す。Q2は、水素原子又はアルカリ金属を示す。2つのQ2はそれぞれ同一であっても異なっていてもよい。) (In formula (1), R 1 is a linear alkyl group having 12 carbon atoms, Q 1 is a linear alkyl group having 12 carbon atoms, an alkali metal, or a hydrogen atom. Q 2 is a hydrogen atom or an alkali Indicates a metal.The two Q2s may be the same or different.)
(式(2)中、R2及びR3は直鎖の炭素数12のアルキル基、M1は、水素原子又はアルカリ金属を示す。) (In formula (2), R 2 and R 3 are linear alkyl groups having 12 carbon atoms, and M 1 is a hydrogen atom or an alkali metal.)
(式(3)中、R4は直鎖の炭素数12のアルキル基、M2及びM3は、それぞれ独立して、水素原子又はアルカリ金属を示す。) (In formula (3), R 4 is a linear alkyl group having 12 carbon atoms, and M 2 and M 3 each independently represent a hydrogen atom or an alkali metal.)
前記処理剤の不揮発分の1%濃度水溶液のpHが6~8であると好ましい。
前記処理剤の不揮発分に占める防腐剤の重量割合が100ppm以下であると好ましい。
本発明の短繊維は、原料繊維に対して、上記不織布製造用繊維処理剤が付着してなる。
It is preferable that the pH of the 1% concentration aqueous solution of the nonvolatile components of the treatment agent is 6 to 8.
Preferably, the weight ratio of the preservative to the nonvolatile content of the processing agent is 100 ppm or less.
The short fibers of the present invention are made by adhering the above-mentioned fiber treatment agent for nonwoven fabric production to raw fibers.
本発明の不織布製造用繊維処理剤が付与した短繊維から製造される不織布は、高温経時後に親水性が低下しない。本発明の短繊維から製造された不織布は、高温経時後に親水性が低下しない。 The nonwoven fabric produced from short fibers to which the fiber treatment agent for nonwoven fabric production of the present invention has been applied does not lose its hydrophilicity after aging at high temperatures. The nonwoven fabric produced from the staple fibers of the present invention does not lose its hydrophilicity after aging at high temperatures.
本発明の不織布製造用繊維処理剤は、化合物(A)、化合物(B)、化合物(C)及び無機燐酸塩(IN)を含む。各化合物について、以下に詳細に説明する。 The fiber treatment agent for nonwoven fabric production of the present invention contains a compound (A), a compound (B), a compound (C), and an inorganic phosphate (IN). Each compound will be explained in detail below.
[化合物(A)]
化合物(A)は、本願発明の不織布製造用繊維処理剤に必須に含まれる成分である。
化合物(A)は、不織布高温経時後の親水性低下を抑制する効果がある。
[Compound (A)]
Compound (A) is an essential component included in the fiber treatment agent for nonwoven fabric production of the present invention.
Compound (A) has the effect of suppressing a decrease in hydrophilicity of a nonwoven fabric after aging at high temperatures.
化合物(A)は、上記一般式(1)で示される。
式中、R1は直鎖の炭素数12のアルキル基である。
Q1は、水素原子、直鎖の炭素数12のアルキル基又はアルカリ金属である。
アルカリ金属としては、カリウム、ナトリウム、リチウム等が挙げられ、不織布高温経時後の親水性低下を抑制する観点から、カリウムが好ましい。
2つのQ2は、それぞれ独立して、水素原子又はアルカリ金属である。
Compound (A) is represented by the above general formula (1).
In the formula, R 1 is a linear alkyl group having 12 carbon atoms.
Q 1 is a hydrogen atom, a linear alkyl group having 12 carbon atoms, or an alkali metal.
Examples of the alkali metal include potassium, sodium, lithium, etc., and potassium is preferred from the viewpoint of suppressing a decrease in hydrophilicity of the nonwoven fabric after aging at high temperatures.
The two Q2 's are each independently a hydrogen atom or an alkali metal.
化合物(A)の具体例としては、特に限定されないが、ピロラウリルホスフェート、ピロラウリルホスフェートカリウム塩、ピロラウリルホスフェートナトリウム塩等が挙げられる。中でも、ピロラウリルホスフェート又はピロラウリルホスフェートカリウム塩が好ましい。 Specific examples of compound (A) include, but are not limited to, pyrrolauryl phosphate, pyrrolauryl phosphate potassium salt, pyrrolauryl phosphate sodium salt, and the like. Among these, pyrrolauryl phosphate or pyrrolauryl phosphate potassium salt is preferred.
化合物(A)は、次のようにして検出することができる。
〔31P-NMR法〕
測定試料不揮発分約30mgを直径5mmのNMR用試料管に秤量し、重水素化溶媒として約0.5mlの重水(D2O)あるいは重クロロホルム(CDCl3)を加え溶解させて、31P-NMR測定装置(BRUKER社製AVANCE400,162MHzおよび日本電子株式会社製JNM-ECZ400R,162MHz)で測定した。
化合物(A)に由来する燐元素のピークは、-5~-15ppmにて検出される。
なお、本発明における不揮発分とは、処理剤を105℃で熱処理して溶媒等を除去し、恒量に達した時の絶乾成分をいう。
Compound (A) can be detected as follows.
[ 31P -NMR method]
Approximately 30 mg of the nonvolatile content of the measurement sample was weighed into a 5 mm diameter NMR sample tube, and approximately 0.5 ml of heavy water (D 2 O) or deuterated chloroform (CDCl 3 ) was added as a deuterated solvent to dissolve the 31 P- Measurement was performed using an NMR measuring device (AVANCE 400, 162 MHz manufactured by BRUKER and JNM-ECZ 400R, 162 MHz manufactured by JEOL Ltd.).
The peak of phosphorus element derived from compound (A) is detected at -5 to -15 ppm.
Note that the nonvolatile content in the present invention refers to an absolutely dry component when a constant weight is reached by heat-treating the processing agent at 105° C. to remove the solvent and the like.
〔化合物(B)〕
化合物(B)は、本願発明の不織布製造用繊維処理剤に必須に含まれる成分であり、化合物(A)及び化合物(C)と併用することにより、不織布高温経時後の親水性低下を抑制する性能を有する。
化合物(B)は、上記一般式(2)で示される。
式中、R2及びR3は直鎖の炭素数12のアルキル基である。
[Compound (B)]
Compound (B) is an essential component included in the fiber treatment agent for producing nonwoven fabrics of the present invention, and when used in combination with compound (A) and compound (C), it suppresses the decrease in hydrophilicity of nonwoven fabrics after aging at high temperatures. Has performance.
Compound (B) is represented by the above general formula (2).
In the formula, R 2 and R 3 are linear alkyl groups having 12 carbon atoms.
M1は、水素原子、アルカリ金属である。
アルカリ金属としては、カリウム、ナトリウム、リチウム等が挙げられ、不織布高温経時後の親水性低下を抑制する観点から、カリウムが好ましい。
M 1 is a hydrogen atom or an alkali metal.
Examples of the alkali metal include potassium, sodium, lithium, etc., and potassium is preferred from the viewpoint of suppressing a decrease in hydrophilicity of the nonwoven fabric after aging at high temperatures.
化合物(B)の具体例としては、特に限定されないが、ジラウリルホスフェート、ジラウリルホスフェートカリウム塩、ジラウリルホスフェートナトリウム塩等が挙げられる。 Specific examples of compound (B) include, but are not limited to, dilauryl phosphate, dilauryl phosphate potassium salt, dilauryl phosphate sodium salt, and the like.
化合物(B)は、化合物(A)と同様に、31P-NMRの方法で検出することができる。
(測定試料不揮発分約30mgを直径5mmのNMR用試料管に秤量し、重水素化溶媒として約0.5mlの重水(D2O)あるいは重クロロホルム(CDCl3)を加え溶解させて、31P-NMR測定装置(BRUKER社製AVANCE400,162MHzおよび日本電子株式会社製JNM-ECZ400R,162MHz)で測定した。)
化合物(B)、後述する化合物(C)及び後述する無機燐酸に由来する燐元素のピークは、+4~-1ppmにて検出される。
化合物(B)、化合物(C)及び無機燐酸に由来する燐元素のピークは、いずれも+4~-1ppmにて検出されるが、低磁場側から、無機燐酸、化合物(C)、化合物(B)の順に帰属が決定される。
Compound (B), like compound (A), can be detected by 31 P-NMR.
(Weigh out about 30 mg of the non-volatile content of the measurement sample into an NMR sample tube with a diameter of 5 mm, add about 0.5 ml of heavy water (D 2 O) or deuterated chloroform (CDCl 3 ) as a deuterated solvent, and dissolve it. 31 P - Measured with NMR measurement equipment (AVANCE 400, 162 MHz manufactured by BRUKER and JNM-ECZ 400R, 162 MHz manufactured by JEOL Ltd.)
The peak of the phosphorus element derived from the compound (B), the compound (C) described later, and the inorganic phosphoric acid described later is detected at +4 to -1 ppm.
The peaks of phosphorus derived from compound (B), compound (C), and inorganic phosphoric acid are all detected at +4 to -1 ppm. ) Attribution is determined in the order of
〔化合物(C)〕
化合物(C)は、本願発明の不織布製造用繊維処理剤に必須に含まれる成分であり、化合物(A)及び化合物(B)と併用することにより、不織布高温経時後の親水性低下を抑制する性能を有する。
化合物(C)は、上記一般式(3)で示される。
式中、R4は直鎖の炭素数12のアルキル基である。
[Compound (C)]
Compound (C) is an essential component included in the fiber treatment agent for producing nonwoven fabrics of the present invention, and when used in combination with compound (A) and compound (B), it suppresses the decrease in hydrophilicity of nonwoven fabrics after aging at high temperatures. Has performance.
Compound (C) is represented by the above general formula (3).
In the formula, R 4 is a linear alkyl group having 12 carbon atoms.
M2は、水素原子又はアルカリ金属である。
アルカリ金属としては、カリウム、ナトリウム、リチウム等が挙げられ、不織布高温経時後の親水性低下を抑制する観点から、カリウム又はナトリウムが好ましい。
M3は、M2と同様である。
M 2 is a hydrogen atom or an alkali metal.
Examples of the alkali metal include potassium, sodium, lithium, etc., and from the viewpoint of suppressing a decrease in hydrophilicity of the nonwoven fabric after aging at high temperatures, potassium or sodium is preferable.
M3 is similar to M2 .
化合物(C)の具体例としては、特に限定されないが、モノラウリルホスフェート、モノラウリルホスフェートモノカリウム塩、モノラウリルホスフェートジカリウム塩、モノラウリルホスフェートモノナトリウム塩、モノラウリルホスフェートジナトリウム塩等が挙げられる。 Specific examples of compound (C) include, but are not limited to, monolauryl phosphate, monopotassium monolauryl phosphate, dipotassium monolauryl phosphate, monosodium monolauryl phosphate, disodium monolauryl phosphate, and the like.
化合物(C)は、化合物(B)と同様に、31P-NMRの方法で検出することができる。
化合物(C)に由来する燐元素のピークは、+4~-1ppmにて検出される。化合物(C)、化合物(B)及び後述する無機燐酸に由来する燐元素のピークは、いずれも+4~-1ppmにて検出されるが、低磁場側から、無機燐酸、化合物(C)、化合物(B)の順に帰属が決定される。
Compound (C), like compound (B), can be detected by 31 P-NMR.
The peak of phosphorus element derived from compound (C) is detected at +4 to -1 ppm. The peaks of phosphorus elements derived from compound (C), compound (B), and inorganic phosphoric acid described below are all detected at +4 to -1 ppm, but from the low magnetic field side, inorganic phosphoric acid, compound (C), and compound Attribution is determined in the order of (B).
〔無機燐酸塩(IN)〕
無機燐酸塩(IN)は、本願発明の不織布製造用繊維処理剤に任意に含まれる成分である。
無機燐酸塩(IN)は、リン酸、リン酸二水素金属塩、リン酸水素二金属塩及びリン酸三金属塩から選ばれる少なくとも一つである。
具体的に、リン酸二水素一金属塩としてはリン酸二水素一カリウム塩、リン酸二水素一ナトリウム塩等が挙げられ、リン酸水素二金属塩としてはリン酸水素二カリウム塩、リン酸水素二ナトリウム塩等が挙げられ、リン酸三金属塩としてはリン酸三カリウム塩、リン酸三ナトリウム塩等が挙げられる。
[Inorganic phosphate (IN)]
Inorganic phosphate (IN) is a component optionally included in the fiber treatment agent for nonwoven fabric production of the present invention.
The inorganic phosphate (IN) is at least one selected from phosphoric acid, metal dihydrogen phosphate, dimetallic hydrogen phosphate, and trimetallic phosphate.
Specifically, monometallic salts of dihydrogen phosphate include monopotassium dihydrogen phosphate, monosodium dihydrogen phosphate, etc., and dimetallic salts of hydrogen phosphate include dipotassium hydrogen phosphate, monopotassium dihydrogen phosphate, etc. Examples include disodium hydrogen salts, and examples of trimetallic phosphates include tripotassium phosphate, trisodium phosphate, and the like.
前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)のそれぞれに帰属されるP核NMR積分値の合計(A+B+C+IN)に対して、前記化合物(A)に帰属されるP核NMR積分値(A)の比率〔A/(A+B+C+IN)〕は、不織布高温経時後の親水性低下を抑制する観点から、20~50%であり、25~48%が好ましく、30~45%がより好ましい。
前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)のそれぞれに帰属されるP核NMR積分値の合計(A+B+C+IN)に対して、前記化合物(B)に帰属されるP核NMR積分値(B)の比率〔B/(A+B+C+IN)〕は、不織布高温経時後の親水性低下を抑制する観点から、20~50%であり、22~48%が好ましく、25~45%がより好ましい。
The compound (A), the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN), relative to the total (A+B+C+IN) of the P-nuclear NMR integral values assigned to each of the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN). The ratio [A/(A+B+C+IN)] of the P-nuclear NMR integral value (A) attributed to the nonwoven fabric is 20 to 50%, preferably 25 to 48%, from the viewpoint of suppressing the decrease in hydrophilicity after aging at high temperature. , 30 to 45% is more preferable.
The compound (B) with respect to the total (A+B+C+IN) of P nuclear NMR integral values assigned to each of the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN). The ratio [B/(A+B+C+IN)] of the P-nuclear NMR integral value (B) assigned to , 25 to 45% is more preferable.
前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)のそれぞれに帰属されるP核NMR積分値の合計(A+B+C+IN)に対して、前記化合物(C)に帰属されるP核NMR積分値(C)の比率〔C/(A+B+C+IN)〕は、20~50%であり、20~45%が好ましく、20~40%がより好ましい。
前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)のそれぞれに帰属されるP核NMR積分値の合計(A+B+C+IN)に対して、前記無機燐酸塩(IN)に帰属されるP核NMR積分値(IN)の比率〔IN/(A+B+C+IN)〕は、不織布高温経時後の親水性低下を抑制する観点から、0~15%であり、0~10%が好ましく、0~5%がより好ましい。
The compound (C) with respect to the total (A+B+C+IN) of the P-nuclear NMR integral values assigned to each of the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN). The ratio [C/(A+B+C+IN)] of the P-nuclear NMR integral value (C) assigned to is 20 to 50%, preferably 20 to 45%, and more preferably 20 to 40%.
With respect to the total (A+B+C+IN) of P-nuclear NMR integral values assigned to each of the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN), the inorganic phosphate ( The ratio [IN/(A+B+C+IN)] of the P-nuclear NMR integral value (IN) attributed to IN) is 0 to 15%, and 0 to 10%, from the viewpoint of suppressing the decrease in hydrophilicity of the nonwoven fabric after high temperature aging. is preferable, and 0 to 5% is more preferable.
処理剤の不揮発分に対して、前記化合物(A)、前記化合物(B)及び前記化合物(C)及び前記無機燐酸塩(IN)の合計重量割合が80~100重量%であり、85~100重量%が好ましく、90~100重量%がさらに好ましい。80重量%未満では、不織布高温経時後の親水性低下を抑制する性能が不足する。 The total weight proportion of the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN) is 80 to 100% by weight, based on the nonvolatile content of the treatment agent, and 85 to 100% by weight. % by weight is preferred, and 90 to 100% by weight is more preferred. If it is less than 80% by weight, the ability to suppress a decrease in hydrophilicity of the nonwoven fabric after aging at high temperatures is insufficient.
〔不織布製造用繊維処理剤〕
本発明の不織布製造用繊維処理剤は、処理剤の安全性の観点から、処理剤の有効濃度0.1%水溶液のBOD値が1~300であると好ましい。処理剤の有効濃度0.1%水溶液のBOD値は、10~290がより好ましく、30~280mg/Lがさらに好ましい。
ここで、BOD値とは、生物化学的酸素要求量のことをいい、ウインクラーアジ化ナトリウム変法に従って測定された値のことである。
[Fiber processing agent for nonwoven fabric production]
The fiber treatment agent for producing nonwoven fabrics of the present invention preferably has a BOD value of 1 to 300 in an aqueous solution with an effective concentration of 0.1% from the viewpoint of the safety of the treatment agent. The BOD value of a 0.1% effective concentration aqueous solution of the treatment agent is more preferably 10 to 290, and even more preferably 30 to 280 mg/L.
Here, the BOD value refers to biochemical oxygen demand, and is a value measured according to a modified Winkler sodium azide method.
本発明の不織布製造用繊維処理剤は、処理剤の不揮発分の酸価(KOHmg/g)が100未満であり、20~60が好ましく、30~50がより好ましい。100を超えると、高温経時後に親水性が不足する。なお、酸価(KOHmg/g)は、次の方法で測定した。
各サンプルを絶乾させ、0.01%フェノールフタレインを溶かしたキシレン/エタノール=1/1溶液50mLに各サンプル1gを溶解させた。当該溶液に0.1mol/L水酸化カリウムエタノール溶液を滴下し、微紅色に呈色するまでの液量(y mL)を測定し、下記計算式より算出した。
x=y×5.61
The fiber treatment agent for producing nonwoven fabrics of the present invention has an acid value (KOHmg/g) of nonvolatile components of the treatment agent of less than 100, preferably 20 to 60, more preferably 30 to 50. If it exceeds 100, hydrophilicity will be insufficient after aging at high temperature. In addition, the acid value (KOHmg/g) was measured by the following method.
Each sample was bone-dried, and 1 g of each sample was dissolved in 50 mL of a 1/1 xylene/ethanol solution containing 0.01% phenolphthalein. A 0.1 mol/L potassium hydroxide ethanol solution was added dropwise to the solution, and the amount of liquid (y mL) until it turned slightly pink was measured, and calculated using the following formula.
x=y×5.61
本発明の不織布製造用繊維処理剤は、不織布高温経時後の親水性低下を抑制する観点から、前記処理剤の不揮発分の1%濃度水溶液のpHが6~8であると好ましい。 In the fiber treatment agent for producing nonwoven fabrics of the present invention, the pH of a 1% concentration aqueous solution of nonvolatile components of the treatment agent is preferably 6 to 8 from the viewpoint of suppressing a decrease in hydrophilicity of the nonwoven fabric after aging at high temperatures.
本発明の不織布製造用繊維処理剤は、不織布高温経時後の親水性低下を抑制する観点から、前記処理剤の不揮発分に占める防腐剤の重量割合が100ppm以下であると好ましく、50ppm以下がより好ましく、20ppm以下がさらに好ましい。 In the fiber treatment agent for producing nonwoven fabrics of the present invention, from the viewpoint of suppressing a decrease in hydrophilicity of the nonwoven fabric after aging at high temperatures, the weight ratio of the preservative to the nonvolatile content of the treatment agent is preferably 100 ppm or less, more preferably 50 ppm or less. It is preferably 20 ppm or less, and more preferably 20 ppm or less.
(その他成分)
本発明の不織布製造用繊維処理剤は、化合物(A)~(C)、無機燐酸以外にも、ノニオン性界面活性剤、化合物(A)~(C)以外のアニオン性界面活性剤を含んでもよい。不織布高温経時後の親水性低下を抑制する観点から、処理剤の不揮発分に対して、ノニオン性界面活性剤、化合物(A)~(C)以外のアニオン性界面活性剤の合計は20重量%以下が好ましい。
ノニオン性界面活性剤としては、下記の化合物(D)、化合物(E)、化合物(F)が挙げられる。
(Other ingredients)
The fiber treatment agent for nonwoven fabric production of the present invention may contain a nonionic surfactant and an anionic surfactant other than the compounds (A) to (C) in addition to the compounds (A) to (C) and inorganic phosphoric acid. good. From the viewpoint of suppressing the decrease in hydrophilicity of the nonwoven fabric after aging at high temperatures, the total amount of anionic surfactants other than the nonionic surfactant and compounds (A) to (C) is 20% by weight based on the nonvolatile content of the treatment agent. The following are preferred.
Examples of the nonionic surfactant include the following compound (D), compound (E), and compound (F).
前記化合物(D)は、1価アルコール、多価アルコールおよびこれらのアルキレンオキシド付加物から選ばれる少なくとも1種と脂肪族カルボン酸とのエステルである。 The compound (D) is an ester of an aliphatic carboxylic acid and at least one selected from monohydric alcohols, polyhydric alcohols, and alkylene oxide adducts thereof.
1価アルコールとしては、特に限定はないが、1価の脂肪族アルコール等が挙げられる。1価の脂肪族アルコールの炭素数は分布があってもよい。また、飽和であっても不飽和あってもよく、直鎖状であってもよく、分岐を有していてもよい。脂肪族アルコールの炭素数は、1~22が好ましく、1~18がより好ましく、4~18がさらに好ましく、8~18が特に好ましい。
1価アルコールとしては、例えば、メタノール、エタノール、ブタノール、2-エチルヘキサノール、ラウリルアルコール、パルミチルアルコール、ステアリルアルコール、イソステアリルアルコール、オレイルアルコール、ベヘニルアルコール等が挙げられる。
1価アルコールのアルキレンオキシド付加物について、アルキレンオキシドの炭素数は2~4が好ましい。2種類以上のアルキレンオキシドを付加する場合、それらの付加順序は特に限定されるものでなく、付加形態はブロック状、ランダム状のいずれでもよい。また、アルキレンオキシドの付加モル数は、0~150が好ましく、0~50がさらに好ましく、0~20が特に好ましく、0が最も好ましい。
Monohydric alcohols include, but are not particularly limited to, monohydric aliphatic alcohols. The number of carbon atoms in the monovalent aliphatic alcohol may be distributed. Further, it may be saturated or unsaturated, linear, or branched. The aliphatic alcohol preferably has 1 to 22 carbon atoms, more preferably 1 to 18 carbon atoms, even more preferably 4 to 18 carbon atoms, and particularly preferably 8 to 18 carbon atoms.
Examples of the monohydric alcohol include methanol, ethanol, butanol, 2-ethylhexanol, lauryl alcohol, palmityl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, and behenyl alcohol.
Regarding the alkylene oxide adduct of monohydric alcohol, the alkylene oxide preferably has 2 to 4 carbon atoms. When two or more types of alkylene oxides are added, the order of their addition is not particularly limited, and the addition form may be either block or random. Further, the number of moles of alkylene oxide added is preferably 0 to 150, more preferably 0 to 50, particularly preferably 0 to 20, and most preferably 0.
多価アルコールとしては、特に限定はないが、2~8価のアルコール等が挙げられ、2~6価のアルコールが好ましく、2~4価のアルコールが好ましい。
多価アルコールとしては、例えば、エチレングリコール、プロピレングリコール、1,4-ブタンジオール、1,6-ヘキサンジオール、ジエチレングリコールなどのジオール類、グリセリン、トリメチロールプロパン、ソルビトール、ソルビタン、ペンタエリスリトール、ショ糖などのポリオール類が挙げられる。さらに、グリセリンの縮合物であるジグリセリン、トリグリセリン、テトラグリセリン、ヘキサグリセリン等のポリグリセリンも含まれる。
多価アルコールのアルキレンオキシドのアルキレンオキシド付加物について、アルキレンオキシドの炭素数は2~4が好ましい。2種類以上のアルキレンオキシドを付加する場合、それらの付加順序は特に限定されるものでなく、付加形態はブロック状、ランダム状のいずれでもよい。また、アルキレンオキシドの付加モル数は、0~150が好ましく、0~50がさらに好ましく、0~20が特に好ましく、0が最も好ましい。
The polyhydric alcohol is not particularly limited, but includes dihydric to octahydric alcohols, preferably dihydric to hexahydric alcohols, and preferably dihydric to tetrahydric alcohols.
Examples of polyhydric alcohols include diols such as ethylene glycol, propylene glycol, 1,4-butanediol, 1,6-hexanediol, and diethylene glycol, glycerin, trimethylolpropane, sorbitol, sorbitan, pentaerythritol, and sucrose. Examples include polyols. Furthermore, polyglycerols such as diglycerin, triglycerin, tetraglycerin, and hexaglycerin, which are condensates of glycerin, are also included.
Regarding the alkylene oxide adduct of an alkylene oxide of a polyhydric alcohol, the alkylene oxide preferably has 2 to 4 carbon atoms. When two or more types of alkylene oxides are added, the order of their addition is not particularly limited, and the addition form may be either block or random. Further, the number of moles of alkylene oxide added is preferably 0 to 150, more preferably 0 to 50, particularly preferably 0 to 20, and most preferably 0.
脂肪族カルボン酸は、分子内にヒドロキシル基を有さない脂肪酸が好ましい。脂肪族カルボン酸としては、特に限定はなく、脂肪酸や脂肪族ポリカルボン酸であってもよい。脂肪酸としては、飽和脂肪酸であってもよく、不飽和脂肪酸であってもよい。これらの中でも、飽和脂肪酸が好ましく、脂肪酸の炭素数は、4~30が好ましく、4~22がさらに好ましく、4~18が特に好ましい。 The aliphatic carboxylic acid is preferably a fatty acid that does not have a hydroxyl group in its molecule. The aliphatic carboxylic acid is not particularly limited, and may be a fatty acid or an aliphatic polycarboxylic acid. The fatty acid may be a saturated fatty acid or an unsaturated fatty acid. Among these, saturated fatty acids are preferred, and the number of carbon atoms in the fatty acid is preferably 4 to 30, more preferably 4 to 22, and particularly preferably 4 to 18.
飽和脂肪酸としては、例えば、カプロン酸、カプリル酸、カプリン酸、ウンデカン酸、ラウリン酸、トリデカン酸、ミリスチン酸、ペンタデカン酸、パルミチン酸、ステアリン酸、ノナデカン酸、アラキジン酸、ベヘン酸、セロチン酸、モンタン酸、メリシン酸等が挙げられる。
不飽和脂肪酸としては、例えば、オレイン酸、エライジン酸、エルカ酸、リノール酸、リノレン酸等が挙げられる。
Examples of saturated fatty acids include caproic acid, caprylic acid, capric acid, undecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, stearic acid, nonadecanoic acid, arachidic acid, behenic acid, cerotic acid, and montanic acid. Examples include acid, melisic acid, and the like.
Examples of unsaturated fatty acids include oleic acid, elaidic acid, erucic acid, linoleic acid, and linolenic acid.
脂肪族ポリカルボン酸としては、例えば、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、スベリン酸、アゼライン酸、セバシン酸、マレイン酸、フマル酸、トリカルバリル酸、クエン酸等が挙げられる。
また、これらの脂肪族ポリカルボン酸無水物も使用することができ、例えば、無水マロン酸、無水コハク酸、無水グルタル酸、無水アジピン酸、無水ピメリン酸、無水スベリン酸、無水アゼライン酸、無水セバシン酸、無水マレイン酸、無水クエン酸等が挙げられる。
Examples of aliphatic polycarboxylic acids include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, maleic acid, fumaric acid, tricarballylic acid, citric acid, etc. can be mentioned.
In addition, these aliphatic polycarboxylic acid anhydrides can also be used, such as malonic anhydride, succinic anhydride, glutaric anhydride, adipic anhydride, pimelic anhydride, suberic anhydride, azelaic anhydride, sebacic anhydride. Examples include acids, maleic anhydride, citric acid anhydride, and the like.
多価アルコールと脂肪酸とのエステルとしては、椰子油、パーム油や大豆油、牛脂などの天然から得られる油脂類、パーム油や大豆油や牛脂に水素を添加した硬化パーム油や硬化大豆油、硬化牛脂等を用いてもよい。 Examples of esters of polyhydric alcohols and fatty acids include naturally occurring fats and oils such as coconut oil, palm oil, soybean oil, and beef tallow; hydrogenated palm oil and hydrogenated soybean oil that are obtained by adding hydrogen to palm oil, soybean oil, and beef tallow; Hardened beef tallow or the like may also be used.
多価アルコールのアルキレンオキシド付加物と脂肪族カルボン酸のエステルとしては、多価アルコールと脂肪族カルボン酸とからエステルを得てから、炭素数2~4のアルキレンオキシドを付加した物質を使用してもよい。 As an ester of an alkylene oxide adduct of a polyhydric alcohol and an aliphatic carboxylic acid, a substance obtained by obtaining an ester from a polyhydric alcohol and an aliphatic carboxylic acid and then adding an alkylene oxide having 2 to 4 carbon atoms is used. Good too.
1価アルコールおよび/または1価アルコールのアルキレンオキシド付加物と脂肪族カルボン酸とのエステルとしては、2-エチルヘキシルオレエート、イソオクチルオレエート、ラウリルオレエート、ステアリルオレエート、オレイルオレエート、トリデシルオレエート、ブチルステアレート、イソオクチルステアレート、オレイルイソステアレート、オレイルステアレート、イソトリデシルステアレート、イソプロピルパルミテート、イソオクチルパルミテート、オレイルパルミテート、トリデシルパルミテート、トリデシルラウレート、オレイルラウレートポリオキシエチレン(10モル)ステアリルエーテルのオレイン酸エステル、ジオクチルアジペート、ジラウリルアジペート、ジイソトリデシルアジペート、ジイソステアリルアジペート、ジオレイルアジペート、ジオクチルフマレート、ジオクチルフタレート等が挙げられる。 Examples of esters of monohydric alcohols and/or alkylene oxide adducts of monohydric alcohols and aliphatic carboxylic acids include 2-ethylhexyl oleate, isooctyl oleate, lauryl oleate, stearyl oleate, oleyl oleate, tridecyl Oleate, butyl stearate, isooctyl stearate, oleyl isostearate, oleyl stearate, isotridecyl stearate, isopropyl palmitate, isooctyl palmitate, oleyl palmitate, tridecyl palmitate, tridecyl laurate, Oleic acid esters of oleyl laurate polyoxyethylene (10 mol) stearyl ether, dioctyl adipate, dilauryl adipate, diisotridecyl adipate, diisostearyl adipate, dioleyl adipate, dioctyl fumarate, dioctyl phthalate, and the like.
多価アルコールおよび/または多価アルコールのアルキレンオキシド付加物と脂肪族カルボン酸とのエステルとしては、エチレングリコールジオレエート、グリセリンモノオクタネート、グリセリンモノデカノエート、グリセリンモノラウレート、グリセリンモノオレエート、グリセリンモノステアレート、グリセリンジオクタネート、グリセリンジデカノエート、グリセリンジラウレート、グリセリントリオレエート、ヘキサグリセリンモノステアレート、トリメチロールプロパントリラウレート、トリメチロールプロパントリオレエート、トリメチロールプロパンモノパルミテート、ペンタエリスリトールテトラオレエート、ソルビタンモノオレエート、ポリオキシエチレン(20モル)グリセリンモノステアレート、ポリオキシエチレン(20モル)ソルビタントリオレエート、コハク酸ジ(3-ヒドロキシプロピル)、コハク酸メチル(3-ヒドロキシプロピル)等が挙げられる。 Examples of esters of polyhydric alcohols and/or alkylene oxide adducts of polyhydric alcohols and aliphatic carboxylic acids include ethylene glycol dioleate, glycerin monooctanate, glycerin monodecanoate, glycerin monolaurate, and glycerin monooleate. ate, glycerin monostearate, glycerin dioctanate, glycerin didecanoate, glycerin dilaurate, glycerin trioleate, hexaglycerin monostearate, trimethylolpropane trilaurate, trimethylolpropane trioleate, trimethylolpropane monopalmitate, Pentaerythritol tetraoleate, sorbitan monooleate, polyoxyethylene (20 mol) glycerin monostearate, polyoxyethylene (20 mol) sorbitan trioleate, di(3-hydroxypropyl) succinate, methyl succinate (3- Hydroxypropyl), etc.
前記化合物(E)は、ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステル(E1)、ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルとジカルボン酸との縮合物(E2)及び当該縮合物(E2)の少なくとも1つの水酸基を脂肪酸で封鎖したエステル(E3)から選ばれる少なくとも1種である。 The compound (E) includes a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester (E1), a condensate of a polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and a dicarboxylic acid (E2), and the condensate (E2) is at least one selected from esters (E3) in which at least one hydroxyl group of the ester is blocked with a fatty acid.
ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステル(E1)は、ポリオキシアルキレン基含有ヒドロキシ脂肪酸と多価アルコールとのエステルであり、多価アルコールの水酸基のうち、2個以上(好ましくは全部)の水酸基がエステル化されている。したがって、ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルは、複数の水酸基を有するエステルである。 The polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester (E1) is an ester of a polyoxyalkylene group-containing hydroxy fatty acid and a polyhydric alcohol, and two or more (preferably all) of the hydroxyl groups of the polyhydric alcohol The hydroxyl group is esterified. Therefore, the polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester is an ester having multiple hydroxyl groups.
ポリオキシアルキレン基含有ヒドロキシ脂肪酸は、脂肪酸の炭化水素基に酸素原子を介してポリオキシアルキレン基が結合した構造を有し、ポリオキシアルキレン基の脂肪酸の炭化水素基と結合していない片末端が水酸基となっている。 Polyoxyalkylene group-containing hydroxy fatty acids have a structure in which a polyoxyalkylene group is bonded to the hydrocarbon group of the fatty acid via an oxygen atom, and one end of the polyoxyalkylene group that is not bonded to the hydrocarbon group of the fatty acid is It is a hydroxyl group.
ヒドロキシ脂肪酸としては、たとえば、ヒドロキシカプリル酸、ヒドロキシカプリン酸、ヒドロキシウンデカン酸、ヒドロキシラウリン酸、ヒドロキシステアリン酸、リシノール酸等が挙げられ、ヒドロキシステアリン酸、リシノール酸が好ましい。
多価アルコールとしては、たとえば、エチレングリコール、グリセリン、トリメチロールプロパン、ソルビタン、ソルビトール、ペンタエリスリトール等が挙げられ、グリセリンが好ましい。
ポリオキシアルキレン基としては、エチレンオキシド、プロピレンオキシド、ブチレンオキシド等の炭素数2~4のアルキレンオキシドが挙げられる。
Examples of the hydroxy fatty acid include hydroxycaprylic acid, hydroxycapric acid, hydroxyundecanoic acid, hydroxylauric acid, hydroxystearic acid, and ricinoleic acid, with hydroxystearic acid and ricinoleic acid being preferred.
Examples of the polyhydric alcohol include ethylene glycol, glycerin, trimethylolpropane, sorbitan, sorbitol, and pentaerythritol, with glycerin being preferred.
Examples of the polyoxyalkylene group include alkylene oxides having 2 to 4 carbon atoms such as ethylene oxide, propylene oxide, and butylene oxide.
ポリオキシアルキレン基含有ヒドロキシ脂肪酸多価アルコールエステルとジカルボン酸との縮合物(E2)を構成するジカルボン酸としては、たとえば、シュウ酸、マロン酸、コハク酸、グルタル酸、アジピン酸、ピメリン酸、スベリン酸、アゼライン酸、セバシン酸、マレイン酸、フマル酸等が挙げられる。 Examples of dicarboxylic acids constituting the condensate (E2) of polyoxyalkylene group-containing hydroxy fatty acid polyhydric alcohol ester and dicarboxylic acid include oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, and suberin. Examples include azelaic acid, sebacic acid, maleic acid, fumaric acid, and the like.
前記縮合物(E2)の少なくとも1つの水酸基を脂肪酸で封鎖したエステル(E3)を構成する封鎖脂肪酸としては、たとえば、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、オレイン酸、イコサン酸、ベヘン酸、リグノセリン酸、ネルボン酸、セロチン酸、モンタン酸、メリシン酸、ラノリン脂肪酸(ウールグリースを精製したラノリン誘導体である炭素数12~36の脂肪酸)等が挙げられる。 Examples of the blocked fatty acids constituting the ester (E3) in which at least one hydroxyl group of the condensate (E2) is blocked with a fatty acid include lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, icosanoic acid, and behenic acid. , lignoceric acid, nervonic acid, cerotic acid, montanic acid, melisic acid, lanolin fatty acid (a fatty acid with 12 to 36 carbon atoms that is a lanolin derivative obtained from refined wool grease), and the like.
前記化合物(F)は、1価の脂肪族アルコールをポリオキシエチレン化して得られる構造を有するアルキルエーテル(以下、POEアルキルエーテル)である。 The compound (F) is an alkyl ether (hereinafter referred to as POE alkyl ether) having a structure obtained by polyoxyethylene-forming a monovalent aliphatic alcohol.
1価の脂肪族アルコールの炭素数については、特に限定はないが、好ましくは8~24、より好ましくは10~20、さらに好ましくは12~18である。
ポリオキシエチレン基1モルを構成するエチレンオキシドの平均付加モル数については、特に限定はないが、好ましくは3~20モル、より好ましくは5~16モル、さらに好ましくは8~12モルである。
The number of carbon atoms in the monohydric aliphatic alcohol is not particularly limited, but is preferably 8 to 24, more preferably 10 to 20, and still more preferably 12 to 18.
The average number of moles of ethylene oxide added per mole of polyoxyethylene group is not particularly limited, but is preferably 3 to 20 moles, more preferably 5 to 16 moles, and even more preferably 8 to 12 moles.
化合物(A)~(C)以外のアニオン性界面活性剤としては、アルキルホスフェート(アルキル基が直鎖の炭素数12であるものを除く)、アルキルホスフェート塩(アルキル基が直鎖の炭素数12であるものを除く)、ポリオキシアルキレン基含有アルキルホスフェート、ポリオキシアルキレン基含有アルキルホスフェート塩、ジアルキルスルホコハク酸およびジアルキルスルホコハク酸塩等が挙げられる。
アルキルホスフェート(アルキル基が直鎖の炭素数12であるものを除く)、アルキルホスフェート塩(アルキル基が直鎖の炭素数12であるものを除く)、ポリオキシアルキレン基含有アルキルホスフェート及びポリオキシアルキレン基含有アルキルホスフェート塩を構成する構成するアルキル基の炭素数としては、本願効果を奏する観点から、6~18(C12を除く)が好ましく、8~16(C12を除く)がより好ましく、8~14(C12を除く)がさらに好ましい。
ジアルキルスルホコハク酸およびジアルキルスルホコハク酸塩を構成する構成するアルキル基の炭素数としては、本願効果を奏する観点から、6~18が好ましく、8~16がより好ましく、8~14がさらに好ましい。
Examples of anionic surfactants other than compounds (A) to (C) include alkyl phosphates (excluding those in which the alkyl group is a straight chain and has 12 carbon atoms), alkyl phosphate salts (excluding those in which the alkyl group is a straight chain and has 12 carbon atoms), ), polyoxyalkylene group-containing alkyl phosphates, polyoxyalkylene group-containing alkyl phosphate salts, dialkyl sulfosuccinic acids, and dialkyl sulfosuccinates.
Alkyl phosphates (excluding those in which the alkyl group is linear and has 12 carbon atoms), alkyl phosphate salts (excluding those in which the alkyl group is linear and has 12 carbon atoms), polyoxyalkylene group-containing alkyl phosphates, and polyoxyalkylene The number of carbon atoms in the alkyl group constituting the group-containing alkyl phosphate salt is preferably 6 to 18 (excluding C12), more preferably 8 to 16 (excluding C12), and more preferably 8 to 16 (excluding C12), from the viewpoint of achieving the effects of the present application. 14 (excluding C12) is more preferred.
The number of carbon atoms in the alkyl group constituting dialkyl sulfosuccinic acid and dialkyl sulfosuccinate is preferably 6 to 18, more preferably 8 to 16, and even more preferably 8 to 14, from the viewpoint of achieving the effects of the present invention.
〔短繊維〕
本発明の短繊維は、不織布製造用合成繊維(原料繊維)とこれに付着した上記不織布製造用繊維処理剤とから構成される短繊維であり、一般的には所定の長さに切断した短い繊維のことである。不織布製造用繊維処理剤の不揮発分の付着率は、前記短繊維に対して0.1~2重量%であり、好ましくは0.3~1重量%である。短繊維に対する不織布製造用繊維処理剤の不揮発分の付着率が0.1重量%未満では、カード工程での制電性が低下し、不織布の地合いが悪化することがある。一方、不織布製造用繊維処理剤の不揮発分の付着率が2重量%を超えると、繊維をカード処理する時に巻付きが多くなって生産性が大幅に低下し、乾式法等の方法により得られた不織布等の繊維製品が透水後にベトツキが大きくなることがある。
[Short fiber]
The short fibers of the present invention are short fibers composed of synthetic fibers for producing nonwoven fabrics (raw fibers) and the above-mentioned fiber treatment agent for producing nonwoven fabrics attached to the synthetic fibers, and are generally short fibers cut into a predetermined length. It refers to fiber. The non-volatile content of the fiber treatment agent for nonwoven fabric production is 0.1 to 2% by weight, preferably 0.3 to 1% by weight, based on the short fibers. If the adhesion rate of the nonvolatile content of the fiber treatment agent for nonwoven fabric production to short fibers is less than 0.1% by weight, the antistatic property in the carding process may be reduced and the texture of the nonwoven fabric may deteriorate. On the other hand, if the non-volatile content of the fiber treatment agent for nonwoven fabric production exceeds 2% by weight, the fibers will become more wrapped when carded, resulting in a significant decrease in productivity, and it will be difficult to obtain fibers obtained by methods such as the dry method. Textile products such as non-woven fabrics may become sticky after water permeates them.
不織布製造用合成繊維(繊維本体)としては、たとえば、ポリオレフィン繊維、ポリエステル繊維、ナイロン繊維、ポリ塩化ビニル繊維、2種類以上の熱可塑性樹脂からなる複合繊維等であり、複合繊維の組み合わせとしては、ポリオレフィン系樹脂/ポリオレフィン系樹脂の場合、例えば、高密度ポリエチレン/ポリプロピレン、直鎖状高密度ポリエチレン/ポリプロピレン、低密度ポリエチレン/ポリプロピレン、プロピレンと他のα-オレフィンとの二元共重合体または三元共重合体/ポリプロピレン、直鎖状高密度ポリエチレン/高密度ポリエチレン、低密度ポリエチレン/高密度ポリエチレン等が挙げられる。また、ポリオレフィン系樹脂/ポリエステル系樹脂の場合、例えば、ポリプロピレン/ポリエチレンテレフタレート、高密度ポリエチレン/ポリエチレンテレフタレート、直鎖状高密度ポリエチレン/ポリエチレンテレフタレート、低密度ポリエチレン/ポリエチレンテレフタレート等が挙げられる。また、ポリエステル系樹脂/ポリエステル系樹脂の場合、例えば、共重合ポリエステル/ポリエチレンテレフタレート、ポリブチレンサクシネート/ポリ乳酸、ポリヒドロキシブチレート/ポリ乳酸、ポリブチレンアジペート・テレフタレート/ポリ乳酸、ポリ乳酸/ポリ乳酸、ポリブチレンサクシネート/ポリブチレンサクシネート等が挙げられる。また、さらにポリアミド系樹脂/ポリエステル系樹脂、ポリオレフィン系樹脂/ポリアミド系樹脂等からなる繊維も例示することができる。不織布製造用繊維処理剤が付着される前の不織布製造用合成繊維は、疎水性合成繊維ということもできる。
これら不織布製造用合成繊維(繊維本体)のなかでも、付着した不織布製造用繊維処理剤が尿や体液等の液体で濡れても繊維表面に残り易いという理由から、ポリオレフィン系繊維(ポリオレフィン繊維やポリオレフィン繊維を含む複合繊維)、ポリエステル系繊維(ポリエステル繊維やポリエステル繊維を含む複合繊維)等の不織布製造用合成繊維に本発明の不織布製造用繊維処理剤は好適である。
Examples of synthetic fibers (fiber main body) for producing nonwoven fabrics include polyolefin fibers, polyester fibers, nylon fibers, polyvinyl chloride fibers, composite fibers made of two or more types of thermoplastic resins, etc. Combinations of composite fibers include: In the case of polyolefin resins/polyolefin resins, for example, high density polyethylene/polypropylene, linear high density polyethylene/polypropylene, low density polyethylene/polypropylene, binary copolymers or terpolymers of propylene and other α-olefins. Examples include copolymer/polypropylene, linear high-density polyethylene/high-density polyethylene, and low-density polyethylene/high-density polyethylene. In the case of polyolefin resin/polyester resin, examples thereof include polypropylene/polyethylene terephthalate, high density polyethylene/polyethylene terephthalate, linear high density polyethylene/polyethylene terephthalate, and low density polyethylene/polyethylene terephthalate. In the case of polyester resin/polyester resin, for example, copolymerized polyester/polyethylene terephthalate, polybutylene succinate/polylactic acid, polyhydroxybutyrate/polylactic acid, polybutylene adipate terephthalate/polylactic acid, polylactic acid/poly Examples include lactic acid, polybutylene succinate/polybutylene succinate, and the like. Furthermore, fibers made of polyamide resin/polyester resin, polyolefin resin/polyamide resin, etc. can also be exemplified. The synthetic fibers for producing nonwoven fabrics before the fiber treatment agent for producing nonwoven fabrics is attached can also be called hydrophobic synthetic fibers.
Among these synthetic fibers (fiber bodies) for manufacturing nonwoven fabrics, polyolefin fibers (polyolefin fibers and The fiber treatment agent for producing nonwoven fabrics of the present invention is suitable for synthetic fibers for producing nonwoven fabrics, such as composite fibers containing fibers) and polyester fibers (composite fibers containing polyester fibers).
繊維の断面構造は鞘芯型、並列型、偏心鞘芯型、多層型、放射型あるいは海島型が例示できるが、繊維製造工程での生産性や、不織布加工の容易さから、偏心を含む鞘芯型または並列型が好ましい。また、断面形状は円形または異形形状とすることができる。異形形状の場合、例えば扁平型、三角形~八角形等の多角型、T字型、中空型、多葉型等の任意の形状とすることができる。 Examples of fiber cross-sectional structures include sheath-core type, parallel type, eccentric sheath-core type, multilayer type, radial type, and sea-island type. Core type or parallel type is preferred. Further, the cross-sectional shape can be circular or irregularly shaped. In the case of an irregular shape, it can be any shape such as a flat shape, a polygonal shape such as a triangular to octagonal shape, a T-shape, a hollow shape, and a multi-lobed shape.
本発明の不織布製造用繊維処理剤は、そのまま希釈等せずに繊維本体に付着させてもよく、水等で不揮発分全体の重量割合が0.5~5重量%となる濃度に希釈してエマルジョンとして繊維本体に付着させてもよい。不織布製造用繊維処理剤を繊維本体へ付着させる工程は、繊維本体の紡糸工程、延伸工程、捲縮工程等のいずれであってもよい。本発明の不織布製造用繊維処理剤を繊維本体に付着させる手段については、特に限定はなく、ローラー給油、ノズルスプレー給油、ディップ給油等の手段を使用してもよい。繊維の製造工程やその特性に合わせ、より均一に効率よく目的の付着量が得られる方法を採用すればよい。また、不織布製造用繊維処理剤が付与された繊維の乾燥の方法としては、熱風および赤外線により乾燥させる方法、熱源に接触させて乾燥させる方法等を用いてよい。 The fiber treatment agent for producing nonwoven fabrics of the present invention may be applied to the fiber body as is without dilution, or it may be diluted with water etc. to a concentration such that the weight ratio of the entire non-volatile content is 0.5 to 5% by weight. It may be applied to the fiber body as an emulsion. The process of attaching the fiber treatment agent for nonwoven fabric production to the fiber body may be any of the spinning process, stretching process, crimping process, etc. of the fiber body. There is no particular limitation on the means for attaching the fiber treatment agent for nonwoven fabric production of the present invention to the fiber body, and means such as roller oiling, nozzle spray oiling, dip oiling, etc. may be used. Depending on the fiber manufacturing process and its characteristics, a method that can more uniformly and efficiently obtain the desired amount of adhesion may be adopted. Further, as a method for drying the fibers to which the fiber treatment agent for nonwoven fabric production has been applied, a method of drying with hot air and infrared rays, a method of drying by contacting with a heat source, etc. may be used.
〔不織布の製造方法〕
不織布の製造方法として、特に限定なく、公知の方法を採用できる。原料繊維としては短繊維や長繊維を用いることができる。原料繊維が短繊維のウェブ形成方式としては、カード方式やエアレイド方式等の乾式法や抄紙方式等の湿式法が挙げられる。また原料繊維が長繊維のウェブ形成方式としては、スパンボンド法、メルトブロー法、フラッシュ紡糸法等が挙げられる。また、繊維間結合方式としては、ケミカルボンド法、サーマルボンド法、ニードルパンチ法、スパンレース法、スティッチボンド法等が挙げられる。
不織布の製造方法は、本発明の短繊維(例えば短繊維)をカード機等に通し繊維ウェブを作製し、得られた繊維ウェブを熱処理する工程を含むものが好ましい。すなわち、本発明の不織布製造用繊維処理剤は、不織布の製造において繊維ウェブを熱処理する工程を有する場合に、特に好適に使用されるものである。
繊維ウェブを熱処理して接合させる方法としては、加熱ロールまたは超音波による熱圧着、加熱空気による熱融着、熱圧着点(ポイントボンディング)法等の熱融着法が挙げられる。繊維ウェブを熱処理して接合させる一例としては、芯に高融点の樹脂を使用し鞘に低融点の樹脂を使用する鞘芯型の複合繊維の場合、低融点の樹脂の融点付近で熱処理することで、繊維交点の熱接着を容易に行なうことができる。
熱接着させる工程を含む不織布の製造方法としては、不織布製造用繊維処理剤が付与された短繊維をカード機等に通しウェブとしたものを上述のように熱処理して接合させ一体化する方法、エアレイド法でパルプ等を積層する際に本発明の短繊維(短繊維)と混綿して、上述のように熱処理して接合させる方法等も挙げられる。その他、スパンボンド法、メルトブロー法、フラッシュ紡糸法等により得られた繊維成形体に対して、本発明の不織布製造用繊維処理剤を付着させたものを加熱ロールまたは加熱空気等で熱処理して、または加熱ロールまたは加熱空気等で熱処理したものに本発明の不織布製造用繊維処理剤を付着させて、不織布を製造する方法も挙げられる。
[Method for manufacturing nonwoven fabric]
There are no particular limitations on the method for producing the nonwoven fabric, and any known method can be employed. Short fibers or long fibers can be used as raw material fibers. Examples of the web forming method using short fibers as raw material include dry methods such as a card method and air-laid method, and wet methods such as a papermaking method. Examples of methods for forming a web in which the raw material fibers are long fibers include a spunbond method, a melt blow method, and a flash spinning method. Examples of the interfiber bonding method include a chemical bond method, a thermal bond method, a needle punch method, a spunlace method, and a stitch bond method.
Preferably, the method for producing a nonwoven fabric includes a step of passing the short fibers (for example short fibers) of the present invention through a carding machine or the like to produce a fibrous web, and heat-treating the obtained fibrous web. That is, the fiber treatment agent for producing a nonwoven fabric of the present invention is particularly preferably used when producing a nonwoven fabric includes a step of heat treating a fibrous web.
Examples of methods for bonding fiber webs by heat treatment include heat bonding methods such as thermocompression bonding using heated rolls or ultrasonic waves, heat fusion bonding using heated air, and thermocompression point bonding methods. As an example of bonding fiber webs by heat treatment, in the case of a sheath-core type composite fiber in which a high melting point resin is used for the core and a low melting point resin for the sheath, heat treatment is performed near the melting point of the low melting point resin. This makes it easy to thermally bond fiber intersections.
A method for manufacturing a nonwoven fabric that includes a step of thermally bonding includes a method in which short fibers to which a fiber treatment agent for nonwoven fabric production has been applied are passed through a card machine or the like to form a web, which is then heat treated as described above and bonded and integrated; When laminating pulp or the like by an air-laid method, a method of mixing the short fibers of the present invention (short fibers) and heat-treating and bonding the fibers as described above is also exemplified. In addition, a fiber molded article obtained by a spunbond method, a melt blow method, a flash spinning method, etc. is coated with the fiber treatment agent for producing a nonwoven fabric of the present invention, and then heat treated with a heated roll or heated air. Alternatively, there is also a method of producing a nonwoven fabric by attaching the fiber treatment agent for nonwoven fabric production of the present invention to a fabric that has been heat treated with a heated roll or heated air.
スパンボンド法の一例としては、複合繊維樹脂を紡糸し、次に、紡出された複合長繊維フィラメントを冷却流体により冷却し、延伸空気によってフィラメントに張力を加えて所期の繊度とする。その後、紡糸されたフィラメントを捕集ベルト上に捕集し、接合処理を行ってスパンボンド不織布を得る。接合手段としては、加熱ロールまたは超音波による熱圧着、加熱空気による熱融着、熱圧着点(ポイントボンディング)法等がある。
得られたスパンボンド不織布に本発明の不織布製造用繊維処理剤を付与する方法としては、グラビア法、フレキソ法、ゲートロール法等のロールコーティング法、スプレーコーティング法等で行うことができるが、不織布への塗布量を片面ずつ調節できるものであれば特に限定されるものではない。また、不織布製造用繊維処理剤が付与された不織布の乾燥の方法としては、熱風および赤外線により乾燥させる方法、熱源に接触させて乾燥させる方法等を用いてよい。
As an example of the spunbond method, a composite fiber resin is spun, and then the spun composite long fiber filament is cooled with a cooling fluid, and tension is applied to the filament with drawing air to obtain the desired fineness. Thereafter, the spun filaments are collected on a collection belt and subjected to a joining treatment to obtain a spunbond nonwoven fabric. Bonding means include thermocompression bonding using heated rolls or ultrasonic waves, heat fusion using heated air, thermocompression point bonding, and the like.
The fiber treatment agent for nonwoven fabric production of the present invention can be applied to the obtained spunbond nonwoven fabric by a gravure method, a flexography method, a roll coating method such as a gate roll method, a spray coating method, etc. There is no particular limitation as long as the amount of coating can be adjusted for each side. Further, as a method for drying the nonwoven fabric to which the fiber treatment agent for nonwoven fabric production has been applied, a method of drying with hot air and infrared rays, a method of drying by contacting with a heat source, etc. may be used.
本発明の不織布において、透水性を発揮する対象の液体としては、尿、軟便、泥状便、水様便、血液、体液、滲出液等が挙げられる。本発明の不織布の用途としては、乳児用使い捨ておむつ、介護用使い捨ておむつ、生理用品、包帯、絆創膏、消毒布、サージカルテープ等の衛生材料用途、ペット用排泄シート、芳香剤の吸液芯、液体防虫剤の吸液芯、清掃布等の日用品用途、コーヒーフィルター、水切りシート等の食品関連用途等が挙げられる。 In the nonwoven fabric of the present invention, examples of liquids that exhibit water permeability include urine, soft stool, muddy stool, watery stool, blood, body fluid, exudate, and the like. The nonwoven fabric of the present invention can be used for sanitary materials such as disposable diapers for infants, disposable diapers for nursing care, sanitary products, bandages, adhesive plasters, disinfectant cloths, and surgical tape, excretory sheets for pets, liquid absorbent cores for air fresheners, and liquid insect repellents. Examples include liquid-absorbing cores for agents, daily necessities such as cleaning cloths, and food-related applications such as coffee filters and draining sheets.
以下に本発明を実施例によって説明するが、本発明はこれに限定されるものではない。尚、各実施例、比較例における評価項目と評価方法は以下の通りである。又、各実施例、比較例における処理剤の明細と評価結果を表1及び2にまとめて示す。処理剤の明細中、配合比率はいずれも重量%を表す。なお、実施例及び比較例において、不織布製造用繊維処理剤の各特性の評価は次の方法に従って行った。 The present invention will be explained below with reference to examples, but the present invention is not limited thereto. The evaluation items and evaluation methods for each example and comparative example are as follows. Further, the details and evaluation results of the processing agents in each Example and Comparative Example are summarized in Tables 1 and 2. In the specification of the processing agent, all compounding ratios represent weight %. In addition, in the Examples and Comparative Examples, evaluation of each characteristic of the fiber treatment agent for nonwoven fabric production was performed according to the following method.
[1重量%水溶液のpH]
各不織布製造用繊維処理剤を濃度が1重量%となるようにイオン交換水で希釈し、pHメーターで水溶液のpHを測定した。
[pH of 1% by weight aqueous solution]
Each fiber treatment agent for nonwoven fabric production was diluted with ion-exchanged water to a concentration of 1% by weight, and the pH of the aqueous solution was measured using a pH meter.
[BOD]
(ウインクラーアジ化ナトリウム変法)
排水を溶存酸素の飽和した希釈水で適量に希釈したものをフ卵瓶に入れ密栓して、5日間×20℃の恒温室で放置し、その前後の溶存酸素量の差から処理剤の有効濃度0.1%水溶液のBODを算出した。実施例1のBODは、270mg/L、実施例7のBODは、292mg/L、比較例1のBODは、311mg/Lであった。
[BOD]
(Modified Winkler sodium azide method)
The wastewater was diluted with an appropriate amount of diluted water saturated with dissolved oxygen, placed in a sealed egg bottle, and left in a constant temperature room at 20°C for 5 days.The effectiveness of the treatment agent was determined by the difference in dissolved oxygen amount before and after. The BOD of an aqueous solution with a concentration of 0.1% was calculated. The BOD of Example 1 was 270 mg/L, the BOD of Example 7 was 292 mg/L, and the BOD of Comparative Example 1 was 311 mg/L.
[製綿工程]
(スカム発生の有無)
製綿工程のスカム発生の代用評価として、ポリエステルフィラメントを用いてスカム評価を行った。
各不織布製造用繊維処理剤の有効10%濃度エマルションを市販のポリエステルフィラメント(200d/24f)の脱脂糸に定量ポンプを用いて、OPU=1.0%となるように給油した。
各不織布製造用繊維処理剤付着糸を40mmφ梨地クロムピン上、糸速度200m/分、入張力25g、接触角180度で一定長(10000m)走行させたときのピン上に蓄積するスカムの有無を肉眼で判定した。3以上であると実用に供し得る。
〔判定基準〕
5 … スカム発生が見られない
4 … スカム発生が僅かに見られる
3 … スカムが少し発生する
2 … スカム発生が見られる
1 … スカムの発生が多く見られる
[Cotton manufacturing process]
(Presence or absence of scum)
As a substitute evaluation for scum generation in the cotton manufacturing process, scum evaluation was performed using polyester filament.
An effective 10% concentration emulsion of each fiber treatment agent for nonwoven fabric production was applied to a commercially available degreased polyester filament (200d/24f) thread using a metering pump so that OPU=1.0%.
When each fiber treatment agent-attached yarn for nonwoven fabric manufacturing is run over a 40 mm diameter satin chrome pin for a constant length (10,000 m) at a yarn speed of 200 m/min, an input tension of 25 g, and a contact angle of 180 degrees, the presence or absence of scum that accumulates on the pin is visually observed. It was judged. If it is 3 or more, it can be put to practical use.
〔Judgment criteria〕
5...No scum formation is observed 4...Scum formation is slightly observed 3...Scum is slightly formed 2...Scum formation is observed 1...Scum formation is observed in large numbers
[カード工程]
(制電性)
カード試験機を用いて20℃×45%RHの条件で試料短繊維40gをシリンダー回転数970rpm(設定可能な最高回転数)でミニチュアカード機に通す。発生した静電気の電圧を測定し、以下の基準で評価する。なお、5が最も良い評価であり、3以上であると実用に供し得る。
5 … 0.5kV未満
4 … 0.5~1.0kV
3 … 1.0kV超~1.5kV、
2 … 1.5kV超~2.0kV
1 … 2.0kVより大
(シリンダー巻付き)
カード試験機を用いて30℃×70%RHの条件で試料短繊維40gをカーディングした後にシリンダーを観察し、以下の基準で評価した。なお、5が最も良い評価である。4以上であると実用に供し得る。
5 … 巻付きなし
4 … 巻付いているが、巻付がシリンダー面の1/10以下に巻付きあり
3 … 巻付がシリンダー面の1/10超かつ1/5以下に巻付きあり
2 … 巻付がシリンダー面の1/5超かつ1/3以下に巻付きあり
1 … 巻付がシリンダー面の1/3超~全面に巻付きあり
[Card process]
(Antistatic property)
Using a card testing machine, 40 g of sample short fibers are passed through a miniature card machine at a cylinder rotation speed of 970 rpm (maximum settable rotation speed) under conditions of 20° C. x 45% RH. Measure the voltage of the static electricity generated and evaluate it using the following criteria. Note that 5 is the best evaluation, and 3 or more can be used for practical purposes.
5... Less than 0.5kV 4... 0.5 to 1.0kV
3... More than 1.0kV to 1.5kV,
2...More than 1.5kV to 2.0kV
1...More than 2.0kV (with cylinder winding)
After carding 40 g of sample short fibers under the conditions of 30° C. and 70% RH using a card testing machine, the cylinder was observed and evaluated based on the following criteria. Note that 5 is the best evaluation. If it is 4 or more, it can be put to practical use.
5... No winding 4... Wound, but less than 1/10 of the cylinder surface is wrapped 3... More than 1/10 and less than 1/5 of the cylinder surface is wrapped 2... Wrapping is more than 1/5 and less than 1/3 of the cylinder surface 1 ... Wrapping is more than 1/3 and the entire surface of the cylinder is wrapped
(不織布の耐久透水性)
EDANA法のRepeated Liquid Strike-Through Time法に従い、不織布(10cm×10cm)に0.9%生理食塩水を透水させ、透水時間を測定した。透水後、不織布を2枚の濾紙(東洋濾紙、No.5)の間に挟み、その上に板(10cm×10cm)と重り(500g)を乗せて3分間放置して脱水し、その後さらに5分間風乾した。
試験に供した不織布について、同様の作業を繰り返して行う。この繰り返し試験では回数を重ねても透水時間が短い方がよい。時間(秒数)を以下の基準で評価する。なお、5が最も良い評価であり、3以上であると実用に供し得る。
〔判定基準〕
5 … 2秒未満
4 … 2秒以上3秒未満
3 … 3秒以上5秒未満
2 … 5秒以上10秒未満
1 … 10秒以上
(Durable water permeability of nonwoven fabric)
According to the Repeated Liquid Strike-Through Time method of the EDANA method, 0.9% physiological saline was permeated through a nonwoven fabric (10 cm x 10 cm), and the water permeation time was measured. After water permeation, the nonwoven fabric was sandwiched between two pieces of filter paper (Toyo Roshi, No. 5), a plate (10 cm x 10 cm) and a weight (500 g) were placed on top of it, and left for 3 minutes to dehydrate. Air dried for a minute.
The same operation is repeated on the nonwoven fabric used in the test. In this repeated test, it is better if the water permeation time is shorter even if the number of times is increased. Evaluate time (seconds) using the following criteria. Note that 5 is the best evaluation, and 3 or more can be used for practical purposes.
〔Judgment criteria〕
5...Less than 2 seconds4...2 seconds or more and less than 3 seconds3...3 seconds or more and less than 5 seconds2...5 seconds or more and less than 10 seconds1...10 seconds or more
[透水性の経時安定性]
不織布(10cm×10cm)を40℃×70%RHの環境試験器に30日放置する。この不織布を30日後に環境試験器から取り出して、上記に示した不織布の耐久透水性試験を行う。環境試験器投入前後の耐久透水性の差が小さいほど、透水性の経時低下が小さいとする。この経時低下が小さい方がよい。
[Water permeability stability over time]
The nonwoven fabric (10 cm x 10 cm) was left in an environmental test chamber at 40°C x 70% RH for 30 days. After 30 days, the nonwoven fabric was taken out of the environmental tester and subjected to the above-mentioned durable water permeability test. It is assumed that the smaller the difference in durable water permeability before and after being placed in the environmental test chamber, the smaller the decrease in water permeability over time. The smaller this decrease over time, the better.
なお、表1~4中に示す成分は次の通りである。なお、表3~4に示すP-1~P-9及びp1~p-3は、表1及び2に示すモル比率で含有する。
(P-1~9、p-3の製造方法)
500mL四つ口フラスコにn-ドデシルアルコール(花王株式会社製、カルコール2098)150gを加えて撹拌しながら、10酸化4リンを総量50gになるように徐々に加えて80℃にて反応させた。得られた未中和物の酸価を測定した。
その後、未中和物の酸価及び目標酸価から算出した必要な水酸化カリウム水溶液に未中和物を滴下し、得られた反応物の酸価を測定した。P核NMR積分値を測定し、化合物(A)、化合物(B)、化合物(C)、及び無機燐酸塩(IN)の帰属を行った。
The components shown in Tables 1 to 4 are as follows. Note that P-1 to P-9 and p1 to p-3 shown in Tables 3 to 4 are contained in the molar ratios shown in Tables 1 and 2.
(Production method of P-1 to 9, p-3)
150 g of n-dodecyl alcohol (Calcol 2098, manufactured by Kao Corporation) was added to a 500 mL four-necked flask, and while stirring, tetraphosphorus 10 oxide was gradually added to a total amount of 50 g, and the mixture was reacted at 80°C. The acid value of the obtained unneutralized product was measured.
Thereafter, the unneutralized product was added dropwise to the necessary potassium hydroxide aqueous solution calculated from the acid value of the unneutralized product and the target acid value, and the acid value of the resulting reaction product was measured. The P-nuclear NMR integral value was measured, and compound (A), compound (B), compound (C), and inorganic phosphate (IN) were assigned.
(p-1の製造方法)
500mL四つ口フラスコにn-ドデシルアルコール(花王株式会社製、カルコール2098)200gを加えて撹拌しながら、10酸化4リンを総量54gになるように徐々に加えて、80℃にて反応させた。得られた未中和物の酸価を測定した。
その後、未中和物の酸価及び目標酸価から算出した必要な水酸化カリウム水溶液に未中和物を滴下し、得られた反応物の酸価を測定した。P核NMR積分値を測定し、化合物(A)、化合物(B)、化合物(C)、及び無機燐酸塩(IN)の帰属を行った。
(Production method of p-1)
200 g of n-dodecyl alcohol (Calcol 2098, manufactured by Kao Corporation) was added to a 500 mL four-necked flask, and while stirring, tetraphosphorus 10 oxide was gradually added to a total amount of 54 g, and the mixture was reacted at 80°C. . The acid value of the obtained unneutralized product was measured.
Thereafter, the unneutralized product was added dropwise to the necessary potassium hydroxide aqueous solution calculated from the acid value of the unneutralized product and the target acid value, and the acid value of the resulting reaction product was measured. The P-nuclear NMR integral value was measured, and compound (A), compound (B), compound (C), and inorganic phosphate (IN) were assigned.
(p-2の製造方法)
500mL四つ口フラスコにn-ドデシルアルコール(花王株式会社製、カルコール2098)250gを加えて撹拌しながら、水を11g仕込み、攪拌した。次に、10酸化4リンを総量90gになるように徐々に加えて反応させた。水を40g加え、さらに80℃で1時間攪拌する。得られた未中和物の酸価を測定した。
その後、未中和物の酸価及び目標酸価から算出した必要な水酸化カリウム水溶液に未中和物を滴下し、得られた反応物の酸価を測定した。P核NMR積分値を測定し、化合物(A)、化合物(B)、化合物(C)、及び無機燐酸塩(IN)の帰属を行った。
(Production method of p-2)
250 g of n-dodecyl alcohol (Calcol 2098, manufactured by Kao Corporation) was added to a 500 mL four-necked flask, and while stirring, 11 g of water was charged and stirred. Next, tetraphosphorus 10 oxide was gradually added to a total amount of 90 g to cause a reaction. Add 40 g of water and stir at 80° C. for 1 hour. The acid value of the obtained unneutralized product was measured.
Thereafter, the unneutralized product was added dropwise to the necessary potassium hydroxide aqueous solution calculated from the acid value of the unneutralized product and the target acid value, and the acid value of the resulting reaction product was measured. The P-nuclear NMR integral value was measured, and compound (A), compound (B), compound (C), and inorganic phosphate (IN) were assigned.
なお、表1~4中に示す成分は次の通りである。なお、表3及び4に示すP-1~P-9及びp1~p-3は、表1及び2に示す積分比率で含有する。
A-1 一般式(1)化合物、R1=n-ドデシル基、Q1:H、K又はn-ドデシル基、Q2:H又はK
B-1 一般式(2)化合物、R2=n-ドデシル基、R3=n-ドデシル基、M1:H又はK
C-1 一般式(3)化合物、R4=n-ドデシル基、M2:H又はK、M3:H又はK、
The components shown in Tables 1 to 4 are as follows. Note that P-1 to P-9 and p1 to p-3 shown in Tables 3 and 4 are contained at the integral ratios shown in Tables 1 and 2.
A-1 Compound of general formula (1), R 1 = n-dodecyl group, Q 1 : H, K or n-dodecyl group, Q 2 : H or K
B-1 Compound of general formula (2), R 2 = n-dodecyl group, R 3 = n-dodecyl group, M 1 : H or K
C-1 compound of general formula (3), R 4 = n-dodecyl group, M 2 : H or K, M 3 : H or K,
化合物D:ポリオキシエチレン(20モル)カスターワックス
化合物E:ポリオキシエチレン(20モル)カスターワックスのマレイン酸縮合物の水酸基1モル当量あたりステアリン酸1モル当量で封鎖したエステル
化合物F:ポリオキシエチレン(7モル)ラウリルアルコール
化合物G:オクチルホスフェート及びオクチルホスフェートカリウム塩(酸価:26)
Compound D: Polyoxyethylene (20 mol) Castor wax Compound E: Polyoxyethylene (20 mol) Ester compound capped with 1 molar equivalent of stearic acid per 1 molar equivalent of hydroxyl group of maleic acid condensate of castor wax F: Polyoxyethylene (7 mol) Lauryl alcohol compound G: octyl phosphate and octyl phosphate potassium salt (acid value: 26)
表3及び4から分かる通り、実施例1~9の不織布製造用繊維処理剤は、前記一般式(1)で示される化合物(A)、前記一般式(2)で示される化合物(B)、前記一般式(3)で示される化合物(C)及び前記無機燐酸塩(IN)から選ばれる少なくとも1種を含む不織布製造用繊維処理剤であって、前記化合物(A)、前記化合物(B)及び前記化合物(C)を必須に含み、
処理剤の不揮発分に対して、前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)の合計重量割合が80~100重量%であり、前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)のそれぞれに帰属されるP核NMR積分値の合計(A+B+C+IN)に対して、前記化合物(A)に帰属されるP核NMR積分値(A)の比率〔A/(A+B+C+IN)〕が20~50%、前記化合物(B)に帰属されるP核NMR積分値(B)の比率〔B/(A+B+C+IN)〕が20~50%、前記化合物(C)に帰属されるP核NMR積分値(C)の比率〔C/(A+B+C+IN)〕が20~50%であり、前記処理剤の不揮発分の酸価(KOHmg/g)が100未満であるため、本願課題を解決できている。
一方、前記化合物(A)に帰属されるP核NMR積分値(A)の比率〔A/(A+B+C+IN)〕が20~50%の範囲にない場合(比較例1~2)、前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)の合計重量割合が100を超える場合(比較例4)、処理剤の不揮発分の酸価(KOHmg/g)が100を超える場合(比較例3)には、高温経時後に親水性が低下しないという本願の課題を解決できていない。
As can be seen from Tables 3 and 4, the fiber treatment agents for producing nonwoven fabrics of Examples 1 to 9 contained a compound (A) represented by the general formula (1), a compound (B) represented by the general formula (2), A fiber treatment agent for producing a nonwoven fabric containing at least one selected from the compound (C) represented by the general formula (3) and the inorganic phosphate (IN), the compound (A) and the compound (B) and essentially contains the compound (C),
The total weight ratio of the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN) is 80 to 100% by weight based on the nonvolatile content of the treatment agent, and the compound ( A), the total of the P-nuclear NMR integral values (A+B+C+IN) assigned to each of the compound (B), the compound (C), and the inorganic phosphate (IN), and the amount assigned to the compound (A). The ratio of the P-nucleus NMR integral value (A) attributed to the compound (B) [A/(A+B+C+IN)] is 20 to 50%, and the ratio of the P-nucleus NMR integral value (B) attributed to the compound (B) [B/(A+B+C+IN)] is 20 to 50%, the ratio [C/(A+B+C+IN)] of the P nuclear NMR integral value (C) assigned to the compound (C) is 20 to 50%, and the acid value of the nonvolatile content of the processing agent ( KOHmg/g) is less than 100, so the problem of the present application can be solved.
On the other hand, when the ratio [A/(A+B+C+IN)] of the P-nucleus NMR integral value (A) assigned to the compound (A) is not in the range of 20 to 50% (Comparative Examples 1 to 2), the compound (A) ), when the total weight ratio of the compound (B), the compound (C) and the inorganic phosphate (IN) exceeds 100 (Comparative Example 4), the acid value (KOHmg/g) of the non-volatile content of the treatment agent is If it exceeds 100 (Comparative Example 3), the problem of the present application that hydrophilicity does not decrease after aging at high temperature cannot be solved.
本発明の不織布製造用繊維処理剤を用いて処理した透水性繊維及び不織布において、透水性を発揮する対象の液体としては、尿、軟便、泥状便、水様便、血液、体液、滲出液等が挙げられる。本発明の不織布の用途としては、乳児用使い捨ておむつ、介護用使い捨ておむつ、生理用品、包帯、絆創膏、消毒布、サージカルテープ等の衛生材料用途、ペット用排泄シート、芳香剤の吸液芯、液体防虫剤の吸液芯、清掃布等の日用品用途、コーヒーフィルター、水切りシート等の食品関連用途等が挙げられる。 In water-permeable fibers and non-woven fabrics treated with the fiber treatment agent for manufacturing non-woven fabrics of the present invention, liquids that exhibit water permeability include urine, soft stool, muddy stool, watery stool, blood, body fluids, and exudates. etc. The nonwoven fabric of the present invention can be used for sanitary materials such as disposable diapers for infants, disposable diapers for nursing care, sanitary products, bandages, adhesive plasters, disinfectant cloths, and surgical tape, excretory sheets for pets, liquid absorbent cores for air fresheners, and liquid insect repellents. Examples include liquid-absorbing cores for agents, daily necessities such as cleaning cloths, and food-related applications such as coffee filters and draining sheets.
Claims (4)
処理剤の不揮発分に対して、前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)の合計重量割合が80~100重量%であり、
前記化合物(A)、前記化合物(B)、前記化合物(C)及び前記無機燐酸塩(IN)のそれぞれに帰属されるP核NMR積分値の合計(A+B+C+IN)に対して、前記化合物(A)に帰属されるP核NMR積分値(A)の比率〔A/(A+B+C+IN)〕が20~50%、前記化合物(B)に帰属されるP核NMR積分値(B)の比率〔B/(A+B+C+IN)〕が20~50%、前記化合物(C)に帰属されるP核NMR積分値(C)の比率〔C/(A+B+C+IN)〕が20~50%であり、
前記処理剤の不揮発分の酸価(KOHmg/g)が100未満である、
不織布製造用繊維処理剤。
The total weight proportion of the compound (A), the compound (B), the compound (C) and the inorganic phosphate (IN) is 80 to 100% by weight with respect to the nonvolatile content of the treatment agent,
The compound (A), the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN), relative to the total (A+B+C+IN) of the P-nuclear NMR integral values assigned to each of the compound (A), the compound (B), the compound (C), and the inorganic phosphate (IN). The ratio [A/(A+B+C+IN)] of the P-nuclear NMR integral value (A) assigned to the compound (B) is 20 to 50%, and the ratio of the P-nuclear NMR integral value (B) assigned to the compound (B) [B/( A+B+C+IN)] is 20 to 50%, and the ratio [C/(A+B+C+IN)] of the P nuclear NMR integral value (C) assigned to the compound (C) is 20 to 50%,
The acid value (KOHmg/g) of the nonvolatile content of the processing agent is less than 100,
Fiber processing agent for nonwoven fabric production.
A short fiber obtained by adhering the fiber treatment agent for producing a nonwoven fabric according to claim 1 or 2 to a raw material fiber.
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